CN103204948A - Method for rapidly extracting polysaccharide from lentinus edodes - Google Patents
Method for rapidly extracting polysaccharide from lentinus edodes Download PDFInfo
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- CN103204948A CN103204948A CN 201210014656 CN201210014656A CN103204948A CN 103204948 A CN103204948 A CN 103204948A CN 201210014656 CN201210014656 CN 201210014656 CN 201210014656 A CN201210014656 A CN 201210014656A CN 103204948 A CN103204948 A CN 103204948A
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Abstract
The invention relates to the field of lentinus edodes, and provides a method for rapidly extracting polysaccharide from lentinus edodes. The method is characterized in that lentinus edodes or stems thereof are subjected to crushing, soaking, flash extracting, extract liquid centrifuging, deproteinizing, micro-filtrating, reverse osmosis, and microwave vacuum drying, such that lentinus edodes polysaccharide is obtained. The method comprises the specific steps that: raw material selection and pretreatment are carried out, wherein dried lentinus edodes or stems thereof are crushed and soaked; flash extracting is carried out, wherein the lentinus edodes soaking liquid is extracted by using a flash extractor; centrifugation is carried out, wherein the extract liquid is centrifuged, such that a supernatant is obtained; deproteinizing is carried out, wherein neutral protease is added into the supernatant, and enzyme-method deproteinizing is carried out; micro-filtrating is carried out, wherein suspended solids such as crude fiber and pectin are removed from the deproteinized liquid by using a 0.2-0.5mum microfiltration membrane; reverse osmosis concentration is carried out, wherein the micro-filtrated liquid is subjected to reverse osmosis concentration; and microwave vacuum drying is carried out, wherein the polysaccharide concentrated liquid is subjected to microwave vacuum drying, such that the lentinus edodes polysaccharide is obtained. The technical scheme provided by the invention has reasonable process configuration, such that operation time is effectively shortened, and operation efficiency is improved. Process linkage automation degree is high, such that semi-continuous operation can be realized. No organic solvent pollution is caused, and the method is environment-friendly. The method has low integral operation energy consumption, and is economical and feasible.
Description
Technical field
The present invention relates to the mushroom field, be a kind of from mushroom the method for rapid extraction polysaccharide.
Background technology
Lentinus Basidiomycetes, Agaricales, Tricholomataceae, Lentinus, formal name used at school Lentinus edodes is the second-biggest-in-the-world edible mushrooms after bisporous mushroom, also is the precious edible mushrooms that China has long enjoyed a good reputation, at the title of among the people have " mountain delicacy ".China's mushroom export trade amount progressively rose in nearly 10 years, occupied more than 80% in the whole world at present, ranked first in the world.The mushroom production of China is at the forefront in the world, contain rich nutrient substances in the mushroom, lentinan wherein, have multiple physiological active functionses such as antitumor, anti-oxidant, antiviral and reducing blood-fat, can be used for preventing and treating multiple disease, therefore be widely used in medicine and health care of food field, both can directly make end product, utilization is absorbed by the body; Also can be used as the intermediate of derived product exploitation, become multiple pharmaceutical and the indispensable raw material of healthcare food product development, therefore, exploitation and the application of lentinan have broad prospects.
The method of extracting about lentinan mainly contains lixiviate, thermal backflow, alkaline process, the extraction of polyoxyethylene glycol method etc. in recent years, assisted extraction method has ultrasonic wave, microwave etc., the method of separation and purification mainly contains adsorption chromatography, ultrafiltration, chromatography etc., and drying means has hot blast, freeze-drying, vacuum-drying etc.Problems of the prior art mainly are summarized as: the excessive introducing of (1) organic solvent; (2) some method manual operation operation more complicated; (3) the treating process cost is too high, causes polysaccharide product to hold at high price, as column chromatography, and links such as chromatographic separation; (4) production cycle long and continuity of operation is poor, influenced output efficiency; Caused the yield reduction when (5) improving purity of polysaccharide.Therefore, utilize the state of the art to be necessary to improve its technology at dried thin mushroom or mushroom handle, develop a kind of fast method that is suitable for rapid scale.
Summary of the invention
Purpose of the present invention just provide a kind of from mushroom the method for rapid extraction polysaccharide, be fit to mass-producing, the efficient lentinan that obtains fast, improved polysaccharide yield simultaneously, kept active polysaccharide to greatest extent.
Technical scheme of the present invention is: the method for polysaccharide in a kind of rapid extraction mushroom is characterized in that: mushroom or mushroom handle through pulverizing, immersion, sudden strain of a muscle formula extract, extracting solution is centrifugal, deproteinated, micro-filtration, reverse osmosis, microwave vacuum drying obtain lentinan; Concrete steps are as follows:
(1) material choice and pre-treatment: get dried thin mushroom or champignon stems, pulverize the back and soak;
(2) sudden strain of a muscle formula is extracted: get the mushroom soak solution and put into flash extracter and extract;
(3) centrifugal: with the centrifugal supernatant liquor that obtains of extracting solution;
(4) deproteinated: add neutral protease in the supernatant liquor and carry out the enzyme process deproteinated;
(5) micro-filtration: deproteinated liquid adopts 0.2-0.5 μ m microfiltration membrane to remove suspended solids such as robust fibre, pectin;
(6) reverse osmosis concentration: the feed liquid of getting after micro-filtration is handled is carried out reverse osmosis concentration;
(7) vacuum microwave drying: the polysaccharide concentrated solution obtains lentinan through vacuum microwave drying.
Material choice is done in the step (1) mushroom or champignon stems, its water content should be lower than 10%, and crushing screening order number is the 30-60 order, adds 10-15 water logging bubble 10-30min doubly;
Extracting rotating speed in the step (2) is 1000-20000r/min, and extraction time 1-3min extracts 2-3 time, and extracting temperature is 20-55 ℃;
Extracting solution is high speed centrifugation under the 3500-6000r/min at rotating speed in the step (3);
The ratio of adding neutral protease in the step (4) in the supernatant liquor is 1%;
Adopt the compound reverse osmosis functional membrane of polymeric amide that feed liquid is concentrated in the step (6), advance film pressure 18-24MPa, advancing film temperature is 30-35 ℃, is concentrated to the 1/5-1/10 of stoste volume;
Adopt vacuum microwave drying in the step (7), vacuum tightness is 3-80Kpa, microwave power 3-15KW, time of drying 30-80min.
Owing to adopt technique scheme, the technical process configuration has rationally been shortened the operating time effectively, has improved operational efficiency; Technology is connected the level of automation height, can realize semicontinuous operation; The pollution of organic solvent-free, environmentally friendly, the overall operation energy consumption is lower simultaneously, economically feasible.
Embodiment
The present invention is further illustrated below in conjunction with embodiment.
Following examples are used for explanation the present invention, but are not used for limiting the scope of the invention.
Embodiment 1
(1) material choice and pre-treatment: get water content≤10% mushroom coarse reduction, crushing screening order number is 60 orders, adds 15 times water logging bubble 30min then;
(2) sudden strain of a muscle formula is extracted: get the mushroom soak solution and put into flash extracter and extract, extraction conditions is 20000r/min for extracting rotating speed, and extraction time 1min extracts 2 times, and the extraction temperature is 20 ℃;
(3) centrifugal: as to be that high speed centrifugation obtains supernatant liquor under the 6000r/min with extracting solution at rotating speed;
(4) deproteinated: adding proportion is that 1% neutral protease carries out the enzyme process deproteinated in the supernatant liquor;
(5) micro-filtration: deproteinated liquid adopts 0.2 μ m microfiltration membrane to remove suspended solids such as robust fibre, pectin;
(6) reverse osmosis concentration: adopt the feed liquid after the compound reverse osmosis functional membrane of polymeric amide is handled micro-filtration to concentrate, advance film pressure 24MPa, advancing film temperature is 30 ℃, is concentrated to 1/5 of stoste volume;
(7) vacuum microwave drying: the polysaccharide concentrated solution is through vacuum microwave drying, and condition is that vacuum tightness is 80Kpa, microwave power 3KW, time of drying 80min.Yield 3.54%, polysaccharide content 94.43%.
Embodiment 2
(1) material choice and pre-treatment: get water content≤10% mushroom coarse reduction, crushing screening order number is 30 orders, adds 10 times water logging bubble 10min then;
(2) sudden strain of a muscle formula is extracted: get the mushroom soak solution and put into flash extracter and extract, extraction conditions is 1000r/min for extracting rotating speed, and extraction time 3min extracts 3 times, and the extraction temperature is 55 ℃;
(3) centrifugal: as to be that high speed centrifugation obtains supernatant liquor under the 3500r/min with extracting solution at rotating speed;
(4) deproteinated: adding proportion is that 1% neutral protease carries out the enzyme process deproteinated in the supernatant liquor;
(5) micro-filtration: deproteinated liquid adopts 0.5 μ m microfiltration membrane to remove suspended solids such as robust fibre, pectin;
(6) reverse osmosis concentration: adopt the feed liquid after the compound reverse osmosis functional membrane of polymeric amide is handled micro-filtration to concentrate, advance film pressure 18MPa, advancing film temperature is 35 ℃, is concentrated to 1/10 of stoste volume;
(7) vacuum microwave drying: the polysaccharide concentrated solution is through vacuum microwave drying, and condition is that vacuum tightness is 3Kpa, microwave power 15KW, time of drying 30min.Acquire lentinan.Yield 3.25%, polysaccharide content 95.12%.
Embodiment 3
(1) material choice and pre-treatment: get water content≤10% champignon stems coarse reduction, crushing screening order number is 40 orders, adds 15 times water logging bubble 25min then;
(2) sudden strain of a muscle formula is extracted: get the champignon stems soak solution and put into flash extracter and extract, extraction conditions is 10000r/min for extracting rotating speed, and extraction time 2min extracts 2 times, and the extraction temperature is 35 ℃;
(3) centrifugal: as to be that high speed centrifugation obtains supernatant liquor under the 5000r/min with extracting solution at rotating speed;
(4) deproteinated: adding proportion is that 1% neutral protease carries out the enzyme process deproteinated in the supernatant liquor;
(5) micro-filtration: deproteinated liquid adopts 0.3 μ m microfiltration membrane to remove suspended solids such as robust fibre, pectin;
(6) reverse osmosis concentration: adopt the feed liquid after the compound reverse osmosis functional membrane of polymeric amide is handled micro-filtration to concentrate, advance film pressure 20MPa, advancing film temperature is 30 ℃, is concentrated to 1/7 of stoste volume;
(7) vacuum microwave drying: the polysaccharide concentrated solution is through vacuum microwave drying, and condition is that vacuum tightness is 50Kpa, microwave power 10KW, time of drying 40min., acquire lentinan.Yield 3.18%, polysaccharide content 91.23%.
Embodiment 4
(1) material choice and pre-treatment: get water content≤10% champignon stems coarse reduction, crushing screening order number is 50 orders, adds 12 times water logging bubble 20min then;
(2) sudden strain of a muscle formula is extracted: get perfume (or spice) and eat the handle soak solution and put into flash extracter and extract, extraction conditions is 8000r/min for extracting rotating speed, and extraction time 3min extracts 3 times, and the extraction temperature is 40 ℃;
(3) centrifugal: as to be that high speed centrifugation obtains supernatant liquor under the 6000r/min with extracting solution at rotating speed;
(4) deproteinated: adding proportion is that 1% neutral protease carries out the enzyme process deproteinated in the supernatant liquor;
(5) micro-filtration: deproteinated liquid adopts 0.4 μ m microfiltration membrane to remove suspended solids such as robust fibre, pectin;
(6) reverse osmosis concentration: adopt the feed liquid after the compound reverse osmosis functional membrane of polymeric amide is handled micro-filtration to concentrate, advance film pressure 24MPa, advancing film temperature is 30 ℃, is concentrated to 1/10 of stoste volume;
(7) vacuum microwave drying: the polysaccharide concentrated solution is through vacuum microwave drying, and condition is that vacuum tightness is 10Kpa, microwave power 7KW, time of drying 60min.Acquire lentinan.Yield 3.16%, polysaccharide content 92.23%.
The present invention has following advantage:
Characteristics of the present invention are that the technical process configuration is reasonable, have shortened the operating time effectively, have improved operational efficiency; Technology is connected the level of automation height, can realize semicontinuous operation; The pollution of organic solvent-free, environmentally friendly, the overall operation energy consumption is lower simultaneously, economically feasible.
(1) adopts sudden strain of a muscle formula extractive technique, based on historrhexis's principle, with high speed machine shearing, stirring, super moving molecule diafiltration technology, in the presence of room temperature and solvent, realize the abundant stripping of effective constituent in several seconds and several minutes, has the heat collapse of not being subjected to, under the solvent load, extraction time is short, the efficient advantages of higher.
(2) adopt the reverse osmosis membrane concentration technique, polysaccharide solution enters reverse osmosis membrane, and the aqueous solvent molecule oozes out under pressure, reaches concentrated purpose.Compare with traditional heating power is concentrated, be characterized in normal-temperature operation, no phase transformation, the thermo-sensitivity composition is protected, and active polysaccharide is kept, and equipment scale is little, energy consumption is low, separation efficiency is high.
(3) because the unusual thickness of polysaccharide concentrated solution, vacuum, lyophilization mode are consuming time longer, the cost height; Warm air drying causes the inside and outside uneven drying of polysaccharide product.Adopt microwave vacuum drying, heat transfer efficiency is higher, and the water in the viscous fluid can directly absorb micro-wave energy and change water vapor under lower temperature; and water vapor is very easily overflowed; can protect the polysaccharide component in the material preferably, advantage such as it is short to have a time of drying, and it is low to consume energy.
Claims (7)
1. the method for a rapid extraction polysaccharide from mushroom is characterized in that: mushroom or mushroom handle through pulverizing, immersion, sudden strain of a muscle formula extract, extracting solution is centrifugal, deproteinated, micro-filtration, reverse osmosis, microwave vacuum drying obtain lentinan; Concrete steps are as follows:
(1) material choice and pre-treatment: get dried thin mushroom or champignon stems, pulverize the back and soak;
(2) sudden strain of a muscle formula is extracted: get the mushroom soak solution and put into flash extracter and extract;
(3) centrifugal: with the centrifugal supernatant liquor that obtains of extracting solution;
(4) deproteinated: add neutral protease in the supernatant liquor and carry out the enzyme process deproteinated;
(5) micro-filtration: deproteinated liquid adopts 0.2-0.5 μ m microfiltration membrane to remove suspended solids such as robust fibre, pectin;
(6) reverse osmosis concentration: the feed liquid of getting after micro-filtration is handled is carried out reverse osmosis concentration;
(7) vacuum microwave drying: the polysaccharide concentrated solution obtains lentinan through vacuum microwave drying;
According to claim 1 a kind of from mushroom the method for rapid extraction polysaccharide, it is characterized in that material choice is done in the step (1) mushroom or champignon stems, its water content should be lower than 10%, and crushing screening order number is the 30-60 order, adds 10-15 water logging bubble 10-30min doubly;
According to claim 1 a kind of from mushroom the method for rapid extraction polysaccharide, it is characterized in that extracting rotating speed in the step (2) is 1000-20000r/min, extraction time 1-3min extracts 2-3 time, the extraction temperature is 20-55 ℃;
According to claim 1 a kind of from mushroom the method for rapid extraction polysaccharide, it is characterized in that extracting solution is high speed centrifugation under the 3500-6000r/min at rotating speed in the step (3);
According to claim 1 a kind of from mushroom the method for rapid extraction polysaccharide, the ratio that it is characterized in that adding in the supernatant liquor in the step (4) neutral protease is 1%;
According to claim 1 a kind of from mushroom the method for rapid extraction polysaccharide, it is characterized in that adopting in the step (6) the compound reverse osmosis functional membrane of polymeric amide that feed liquid is concentrated, advance film pressure 18-24MPa, advancing film temperature is 30-35 ℃, is concentrated to the 1/5-1/10 of stoste volume;
According to claim 1 a kind of from mushroom the method for rapid extraction polysaccharide, it is characterized in that adopting vacuum microwave drying in the step (7), vacuum tightness is 3-80Kpa, microwave power 3-15KW, time of drying 30-80min.
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Cited By (16)
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| CN103788227A (en) * | 2014-01-27 | 2014-05-14 | 河南农业大学 | Extraction method for isatis root polysaccharides |
| CN103864951A (en) * | 2014-03-28 | 2014-06-18 | 河南中医学院 | Preparation method and application of hematoxylon polysaccharide |
| CN104725524A (en) * | 2015-03-31 | 2015-06-24 | 川渝中烟工业有限责任公司 | Method for extracting tobacco polysaccharides from waste tobacco stems in farmlands |
| CN104830537A (en) * | 2015-04-30 | 2015-08-12 | 东莞波顿香料有限公司 | Preparation method and application of aquilaria wood hydrolat |
| CN104886211A (en) * | 2015-05-14 | 2015-09-09 | 湖北省农业科学院农产品加工与核农技术研究所 | Preparation method of pleurotus eryngii and fresh orange fruitcake |
| CN104892791A (en) * | 2015-06-29 | 2015-09-09 | 成都大学 | Lentinan and extraction and purification method thereof |
| CN105111324A (en) * | 2015-08-28 | 2015-12-02 | 武汉工程大学 | Flash extraction method of polysaccharide from Flammulina velutipes leftovers |
| CN104725523B (en) * | 2015-03-31 | 2016-11-09 | 川渝中烟工业有限责任公司 | Utilize the method that homogenate extraction technology discards extraction tobacco polysaccharide fresh tobacco leaf from land for growing field crops |
| CN106832040A (en) * | 2017-04-01 | 2017-06-13 | 高愿军 | A kind of extracting method of lentinan |
| CN107082820A (en) * | 2017-04-25 | 2017-08-22 | 河南省农业科学院 | A kind of method that pulsating negative pressure low temperature extracts lentinan |
| CN107183680A (en) * | 2017-05-09 | 2017-09-22 | 安徽禾泉农庄生态农业有限公司 | A kind of dried thin mushroom processing method |
| CN109942722A (en) * | 2019-03-13 | 2019-06-28 | 江苏盈科生物制药有限公司 | A kind of production method of lentinan |
| CN110122849A (en) * | 2019-05-20 | 2019-08-16 | 辽宁中菊生物科技有限公司 | A kind of preparation method of Shitake Mushroom P.E |
| CN110922498A (en) * | 2019-12-09 | 2020-03-27 | 河南自然之道生物工程有限公司 | Method for preparing lentinan and lentinan polypeptide from defective lentinus edodes and lentinus edodes stems |
| CN113278085A (en) * | 2021-05-24 | 2021-08-20 | 福建宏泰莱生物科技有限公司 | Non-ethanol precipitated high molecular weight tremella polysaccharide and preparation method thereof |
| CN115181192A (en) * | 2022-08-02 | 2022-10-14 | 上海应用技术大学 | Extraction method of echeveria cauliflora stem polysaccharide |
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2012
- 2012-01-11 CN CN 201210014656 patent/CN103204948A/en active Pending
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| CN103864951B (en) * | 2014-03-28 | 2016-03-02 | 河南中医学院 | A kind of preparation method of bush polysaccharide and application |
| CN103864951A (en) * | 2014-03-28 | 2014-06-18 | 河南中医学院 | Preparation method and application of hematoxylon polysaccharide |
| CN104725524A (en) * | 2015-03-31 | 2015-06-24 | 川渝中烟工业有限责任公司 | Method for extracting tobacco polysaccharides from waste tobacco stems in farmlands |
| CN104725523B (en) * | 2015-03-31 | 2016-11-09 | 川渝中烟工业有限责任公司 | Utilize the method that homogenate extraction technology discards extraction tobacco polysaccharide fresh tobacco leaf from land for growing field crops |
| CN104725524B (en) * | 2015-03-31 | 2016-10-19 | 川渝中烟工业有限责任公司 | Utilize the method that homogenate extraction technology extracts Nicotiana tabacum L. polysaccharide from the waste tobacco stem of land for growing field crops |
| CN104830537A (en) * | 2015-04-30 | 2015-08-12 | 东莞波顿香料有限公司 | Preparation method and application of aquilaria wood hydrolat |
| CN104830537B (en) * | 2015-04-30 | 2018-05-18 | 东莞波顿香料有限公司 | A kind of preparation method and applications of agalloch eaglewood hydrosol |
| CN104886211A (en) * | 2015-05-14 | 2015-09-09 | 湖北省农业科学院农产品加工与核农技术研究所 | Preparation method of pleurotus eryngii and fresh orange fruitcake |
| CN104886211B (en) * | 2015-05-14 | 2018-01-23 | 湖北省农业科学院农产品加工与核农技术研究所 | A kind of preparation method of pleurotus eryngii orange fruitcake |
| CN104892791A (en) * | 2015-06-29 | 2015-09-09 | 成都大学 | Lentinan and extraction and purification method thereof |
| CN104892791B (en) * | 2015-06-29 | 2017-05-03 | 成都大学 | Lentinan and extraction and purification method thereof |
| CN105111324A (en) * | 2015-08-28 | 2015-12-02 | 武汉工程大学 | Flash extraction method of polysaccharide from Flammulina velutipes leftovers |
| CN106832040B (en) * | 2017-04-01 | 2019-08-13 | 河南夕阳蓝食品科技有限公司 | A kind of extracting method of lentinan |
| CN106832040A (en) * | 2017-04-01 | 2017-06-13 | 高愿军 | A kind of extracting method of lentinan |
| CN107082820A (en) * | 2017-04-25 | 2017-08-22 | 河南省农业科学院 | A kind of method that pulsating negative pressure low temperature extracts lentinan |
| CN107082820B (en) * | 2017-04-25 | 2019-06-14 | 河南省农业科学院 | A kind of method that pulsating negative pressure low temperature extracts lentinan |
| CN107183680A (en) * | 2017-05-09 | 2017-09-22 | 安徽禾泉农庄生态农业有限公司 | A kind of dried thin mushroom processing method |
| CN109942722A (en) * | 2019-03-13 | 2019-06-28 | 江苏盈科生物制药有限公司 | A kind of production method of lentinan |
| CN110122849A (en) * | 2019-05-20 | 2019-08-16 | 辽宁中菊生物科技有限公司 | A kind of preparation method of Shitake Mushroom P.E |
| CN110922498A (en) * | 2019-12-09 | 2020-03-27 | 河南自然之道生物工程有限公司 | Method for preparing lentinan and lentinan polypeptide from defective lentinus edodes and lentinus edodes stems |
| CN113278085A (en) * | 2021-05-24 | 2021-08-20 | 福建宏泰莱生物科技有限公司 | Non-ethanol precipitated high molecular weight tremella polysaccharide and preparation method thereof |
| CN113278085B (en) * | 2021-05-24 | 2023-01-24 | 福建宏泰莱生物科技有限公司 | Non-ethanol precipitated high molecular weight tremella polysaccharide and preparation method thereof |
| CN115181192A (en) * | 2022-08-02 | 2022-10-14 | 上海应用技术大学 | Extraction method of echeveria cauliflora stem polysaccharide |
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Application publication date: 20130717 |